CN105061526A - Extraction method for high purity rubusoside - Google Patents
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Abstract
The present invention discloses an extraction method for high purity rubusoside. The extraction method comprises the following steps: (1) pre-treatment: removing impurities from a dried sweet tea raw material, and smashing, sieving and obtaining the dried sweet tea raw material to sweet tea raw material powder; (2) microwave counter-current extraction: performing microwave counter-current extraction on the sweet tea raw material, extruding extracted residues, and mixing and filtering an extruding liquid and a sweet tea feed liquid to obtain an extracting liquid; (3) performing centrifugation to obtain centrifugate; (4) macroporous resin adsorptive separation: adjusting the pH value of the centrifugate to 10.0-11.0, passing the centrifugate through macroporous resin for adsorption, and after leaving the centrifugate to stand, performing water-washing and eluting to collect a target eluent; (5) performing ultra-filtration to obtain ultrafiltrate; (6) performing concentration to obtain a concentrate; and (7) crystallization and recrystallization: adding an organic solvent into the concentrate for crystallization, then performing recrystallization and drying to obtain a rubusoside product. According to the rubusoside product obtained by the method provided by the invention, the purity is greater than or equal to 99%, and the yield is greater than or equal to 5.35%. The extraction method provided by the present invention is simple and convenient in process, short in period, low in energy consumption and production cost and can be used for continuous extraction, and is suitable for continuous production in a factory.
Description
Technical field
The present invention relates to a kind of extracting method of Rubusoside, be specifically related to a kind of extracting method being adapted to industrial high purity Rubusoside.
Background technology
Sweet tea be the sweet tea of Rosaceae rubus (
rubusSuatrssimusS.Lee) dry leaf, be mainly distributed in Dayaoshan, Guangxi district, in Guangdong, also there is a small amount of plantation on Hunan, the ground such as Jiangxi.Taste is sweet, there is anti-pollen hypersensitivity, promote the effect such as insulin secretion, prevention and cure of cardiovascular disease, its main component is Rubusoside, its sugariness is about 300 times of sucrose, calorific value is 5% of sucrose, is mainly used as sweeting agent, is widely used in the industry such as food, drink, because it has high sugariness, low-calorie distinguishing feature, quite favor by market.
At present, the domestic research to extracting high purity Rubusoside from sweet tea is rather paid attention to, and pertinent literature report is more.
CN102702284A discloses a kind of production method of high purity Rubusoside, the method be sweet tea raw material carried out extract, concentrate, flocculate and clarify, centrifugal after, again after macroporous resin adsorption separation, ion exchange resin exchange decolouring, desalination, composite decoloration, concentrate drying is prepared into product, product purity reaches 98%, but yield only 3.7 ~ 4.5%, and process is complicated, loss is comparatively large, causes the finished product yield very low.
CN102838644B discloses a kind of production method extracting Rubusoside from sweet tea, the method is that sweet tea raw material is carried out ultrasound assisted extraction, alcohol precipitation, filtration after concentrating under reduced pressure, be separated through macroporous resin adsorption, polyamide resin chromatography, crystallization and recrystallization obtain product, product purity reaches more than 98%, yield about 3.7 ~ 3.9%, the method because of alcohol precipitation not exclusively and polymeric amide wash-out time thorough, cause the yield of the finished product lower.
CN104262425A discloses a kind of novel method extracting Rubusoside, the method is that sweet tea raw material is carried out water extraction, after membrane filtration, cross macroporous resin adsorption separations, zwitterion resin isolation, concentrated, crystallization and recrystallization acquisition product, product purity reaches 99%, yield about 5.31%, the method is because of when macroporous resin adsorption is separated, Reusability acid-alkali treatment, adds subsequent processes, extends the production cycle, also have higher requirement to equipment, production cost is relatively high simultaneously.
CN104558088A discloses a kind of mode utilizing microwave counter current to extract, through cascade filtration, macroporous resin adsorption is separated, membrane filtration, concentrated, dry, the technique of obtained momordica glycoside V 60% product, but when cascade filtration, use and centrifugally to carry out with the mode of multi-ultrafiltration, add process, extend filtration cycle, efficiency is low, energy consumption is large, in addition, after macroporous resin purification, also containing a large amount of impurity, nanofiltration mode is used to carry out inorganic salt and solvent, to reaching concentrated object, in process, pressure is higher, power consumption is large, also larger to the infringement of film, extraction efficiency, process costs aspect is not good yet.
Summary of the invention
Technical problem to be solved by this invention is, overcomes the above-mentioned defect that prior art exists, provides that a kind for the treatment of capacity is large, technique is simple, cost is low, the extracting method of what product purity, yield were high be applicable to industrial high purity Rubusoside.
The technical solution adopted for the present invention to solve the technical problems is as follows: a kind of extracting method of high purity Rubusoside, comprises the following steps:
(1) pre-treatment: by the sweet tea impurity removing of drying, pulverizes, sieves, obtain sweet tea raw material powder;
(2) microwave counter current extracts: sweet for step (1) gained tea raw material powder is carried out microwave counter current extraction, obtains extracting solution;
(3) centrifugal: step (2) gained extracting solution to be carried out centrifugal, obtains centrifugate;
(4) macroporous resin adsorption is separated: by step (3) gained centrifugate adjust ph to 10.0 ~ 11.0, then crosses macroporous resin and carries out upper prop absorption, leave standstill after washing, then carry out wash-out with hydrophilic solvent, collect target elutriant;
(5) ultrafiltration: the target elutriant that step (4) is collected is carried out ultrafiltration, obtains ultrafiltrated;
(6) concentrated: it is 25 ~ 28 that step (5) gained ultrafiltrated is concentrated into hundred sharp degree, obtains concentrated solution;
(7) crystallization and recrystallization: adding organic solvent to the volume fraction of organic solvent in step (6) gained concentrated solution is 80 ~ 90%, then carries out crystallization and recrystallization, dry, obtain Rubusoside product.
Sweet tea raw material used in the present invention originates from Guangxi, and the content of Rubusoside is 6.38 ~ 6.56wt%.
Further, in step (1), described in the order number that sieves be 20 ~ 40 orders.
Further, in step (2), the temperature that described microwave counter current extracts is 70 ~ 90 DEG C, and the time is 40 ~ 60min, and the power of microwave is 700 ~ 900w, and frequency is 5000 ~ 7000MHz; Extraction solvent is deionized water, and consumption is 6 ~ 7 times of sweet tea raw materials quality.This step is different from traditional extracting mode, there is continuous extraction, advantage that treatment capacity is large, this step has the double dominant of microwave extraction and countercurrent extraction, substantially reduce extracting cycle and efficiency, be 1/4 ~ 1/3 of traditional circumfluence distillation technology time, also save the Extraction solvent of more than 30% simultaneously, decrease energy consumption, tradition extraction is the extracting mode of a kind of high-level efficiency, low cost relatively, and the extract yield of this step Rubusoside reaches more than 99%.
Further, in step (3), carry out centrifugal before, extracting solution, first through board frame type heat-exchanger, is cooled to 20 ~ 25 DEG C.
Further, in step (3), described centrifugal elder generation carries out spiral centrifugal with centrifugation rate 3000 ~ 5000r/min, then it is centrifugal to carry out tubular type with centrifugation rate 12000 ~ 14000r/min.Spiral centrifugal is low-speed centrifugal, can eliminate a large amount of particulate matter, and tubular type centrifugal be high speed centrifugation, can be removed by the material that is suspended wherein further, this array mode is compared single centrifugal, ensure that centrifugal continuity, improve centrifugal efficiency, feed liquid is more clarified.
In step (4), before macroporous resin adsorption separation is carried out to centrifugate, need first with alkaline matter, pH value to be adjusted to 10.0 ~ 11.0, object is that the acidic substance in material and most of coloring matter are existed in the form of an ion, thus when carrying out macroporous resin adsorption, can not be adsorbed, and directly flowed out with effluent liquid, to remove most of acidic substance and pigment.Meanwhile, in the basic conditions, can expand slightly in the aperture of macroporous resin, decreases the probability of resin blocking.In addition, when pH value is 10.0 ~ 11.0, Rubusoside material more can be made to exist with molecularity, the salinity in feed liquid increases, and more can increase the adsorptive capacity of resin to Rubusoside.
Further, in step (4), by sodium hydroxide or sodium carbonate adjust ph; Described macroporous resin is D101, AB-8 or DM-130, and the blade diameter length ratio of resin column is 1:4 ~ 6; The flow velocity of described upper prop effluent liquid is 0.5 ~ 1.0BV/h.
Further, in step (4), the described standing time is 2 ~ 3h; During described washing, the flow velocity of water is 2 ~ 3BV/h, be washed to effluent liquid be micro-yellow and pH value is 6.80 ~ 7.20 time till.
Further, in step (4), described hydrophilic solvent is the ethanolic soln of volume fraction 60 ~ 80%, and the elution flow rate of hydrophilic solvent is 0.75 ~ 1.25BV/h, and the elution volume of hydrophilic solvent is 3BV, and collection section is 1.25 ~ 3.0BV.
Further, in step (5), described ultrafiltration adopts rolling ultrafiltration membrane, and the molecular weight cut-off of ultra-filtration membrane is 3000 ~ 5000.Adopt ultrafiltration mainly to remove some protein, tannin and some coloring matters, be further purified material, for later separation is ready.
Further, in step (6), described simmer down to vacuum concentration, temperature is 70 ~ 80 DEG C, and vacuum tightness is-0.06 ~-0.04MPa.
Further, in step (7), described organic solvent is methyl alcohol or ethanol; The temperature of described crystallization and recrystallization is-2 ~ 3 DEG C, and every subcrystalline time is 10 ~ 12h; Described drying is vacuum-drying, and temperature is 50 ~ 60 DEG C, and vacuum tightness is-0.09 ~-0.06MPa, and the time is 12 ~ 16h.Crystallization and recrystallization make use of target component solubleness in organic solvent has higher susceptibility to temperature, and the insensitive different properties of impurity is separated, and reaches good separating effect.
The inventive method has following beneficial effect:
(1) according to the inventive method gained Rubusoside product, purity >=99%, yield >=5.35%, the purity of gained Rubusoside and yield in prior art;
(2) the inventive method before centrifugation, board frame type heat-exchanger is creatively used to reduce rapidly extracting solution temperature, a large amount of normal-temperature water dissolubility sedimentations is separated out, after centrifugal, can remove better, decrease the interference of impurity to subsequent technique, be better purification of target composition, lay a good foundation;
(3) the inventive method carries out alkali tune process before macroporous resin adsorption is separated, eliminate a large amount of acidic substance and pigment, in conjunction with follow-up membrane filtration, eliminate the materials such as pigment further, reach the object of purification of target composition, for next step repurity is got ready, thus instead of the mode of traditional alcohol precipitation, zwitterion plastic resin treatment, technological process is simplified, and further shorten the production cycle;
(4) the inventive method employs microwave counter current extractive technique, instead of traditional circumfluence distillation technology, have extraction time short, use solvent few, energy consumption, production cost are low, and the feature such as to extract continuously, adapt to factory's continuous prodution.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
The sweet tea raw material that the embodiment of the present invention below introduced uses originates from Guangxi; The chromatography column specification used is Ф 400 × 2400mm, and chromatography column material is stainless steel; D101, AB-8 macroporous type polymeric adsorbent, purchased from resin company limited of Shanghai Nankai, DM-130 macroporous type polymeric adsorbent is purchased from Xi'an Lan Xiao novel material limited-liability company; The wavelength that HPLC UV-detector detects is 540nm; Other chemical reagent used and plant and instrument, if no special instructions, all obtained by routine business approach.
embodiment 1
(1) pre-treatment: by sweet for the 500kg of drying tea raw material (Rubusoside content is 6.42%) removal of impurities, pulverizes, and crosses 40 mesh sieves, obtains sweet tea raw material powder;
(2) microwave counter current extracts: by sweet for step (1) gained 500kg tea raw material powder at 90 DEG C, microwave power is 900w, and frequency is under 5000MHz, carries out microwave counter current extract 60min with 3295L deionized water, the flowing of material and water is reverse continuous dynamic flow, obtains 3125kg extracting solution;
(3) centrifugal: by step (2) gained 3125kg extracting solution, 20 DEG C are cooled to rapidly through board frame type heat-exchanger, then first spiral centrifugal is carried out with horizontal spiral centrifuge with centrifugation rate 5000r/min, carry out tubular type with tubular-bowl centrifuge with centrifugation rate 14000r/min more centrifugal, obtain 3120kg centrifugate;
(4) macroporous resin adsorption is separated: by step (3) gained 3120kg centrifugate sodium hydroxide adjust ph to 10.98, then the chromatography column (blade diameter length ratio 1:6) crossing filling D101 macroporous adsorbent resin carries out upper prop absorption, the flow velocity of upper prop effluent liquid is 1.0BV/h, 3h is left standstill after absorption, then wash with deionized water, the flow velocity of deionized water is 3BV/h, being washed to effluent liquid is micro-yellow, and to measure pH value be till 7, wash-out is carried out again with the ethanolic soln that volume fraction is 80%, the elution flow rate of ethanolic soln is 1.25BV/h, the elution volume of ethanolic soln is 3BV, collecting 1.25 ~ 3.0BV section is target elutriant,
(5) ultrafiltration: the target elutriant molecular weight cut-off that step (4) is collected be 5000 rolling ultrafiltration membrane carry out ultrafiltration, obtain ultrafiltrated;
(6) concentrated: by step (5) gained ultrafiltrated at 80 DEG C, vacuum tightness is under-0.06 ~-0.04MPa, and the sharp degree of vacuum concentration to hundred is 25, obtains concentrated solution;
(7) crystallization and recrystallization: adding methyl alcohol to the volume fraction of methyl alcohol in step (6) gained concentrated solution is 90%, then at temperature-2 DEG C, crystallization, repeat crystallization again 1 time, every subcrystalline time is 12h, and by crystal at 60 DEG C, vacuum tightness is under-0.09 ~-0.06MPa, carry out vacuum-drying 16h, obtain Rubusoside product 27.15kg.
Detect through HPLC, the product purity of Rubusoside is 99.08%, and yield is 5.43%.
embodiment 2
(1) pre-treatment: by sweet for the 500kg of drying tea raw material (Rubusoside content is 6.45%) removal of impurities, pulverizes, and crosses 20 mesh sieves, obtains sweet tea raw material powder;
(2) microwave counter current extracts: by sweet for step (1) gained 500kg tea raw material powder at 70 DEG C, microwave power is 900w, and frequency is under 7000MHz, carries out microwave counter current extract 40min with 3298L deionized water, the flowing of material and water is reverse continuous dynamic flow, obtains 3133kg extracting solution;
(3) centrifugal: by step (2) gained 3133kg extracting solution, 25 DEG C are cooled to rapidly through board frame type heat-exchanger, then first spiral centrifugal is carried out with horizontal spiral centrifuge with centrifugation rate 3000r/min, carry out tubular type with tubular-bowl centrifuge with centrifugation rate 12000r/min more centrifugal, obtain 3125kg centrifugate;
(4) macroporous resin adsorption is separated: by step (3) gained 3125kg centrifugate sodium carbonate adjust ph to 10.07, then the chromatography column (blade diameter length ratio 1:4) crossing filling AB-8 macroporous adsorbent resin carries out upper prop absorption, the flow velocity of upper prop effluent liquid is 0.5BV/h, 2h is left standstill after absorption, then wash with deionized water, the flow velocity of deionized water is 2BV/h, being washed to effluent liquid is micro-yellow, and to measure pH value be till 7.02, wash-out is carried out again with the ethanolic soln that volume fraction is 60%, the elution flow rate of ethanolic soln is 0.75BV/h, the elution volume of ethanolic soln is 3BV, collecting 1.25 ~ 3.0BV section is target elutriant,
(5) ultrafiltration: the target elutriant molecular weight cut-off that step (4) is collected be 3000 rolling ultrafiltration membrane carry out ultrafiltration, obtain ultrafiltrated;
(6) concentrated: by step (5) gained ultrafiltrated at 70 DEG C, vacuum tightness is under-0.06 ~-0.04MPa, and the sharp degree of vacuum concentration to hundred is 28, obtains concentrated solution;
(7) crystallization and recrystallization: adding methyl alcohol to the volume fraction of methyl alcohol in step (6) gained concentrated solution is 80%, then at temperature 3 DEG C, crystallization, repeat crystallization again 1 time, each crystallization time is 10h, and by crystal at 50 DEG C, vacuum tightness is under-0.09 ~-0.06MPa, carry out vacuum-drying 12h, obtain Rubusoside product 26.85kg.
Detect through HPLC, the product purity of Rubusoside is 99.37%, and yield is 5.37%.
embodiment 3
(1) pre-treatment: by sweet for the 500kg of drying tea raw material (Rubusoside content is 6.51%) removal of impurities, pulverizes, and crosses 30 mesh sieves, obtains sweet tea raw material powder;
(2) microwave counter current extracts: by sweet for step (1) gained 500kg tea raw material powder at 80 DEG C, microwave power is 800w, and frequency is under 6000MHz, carries out microwave counter current extract 50min with 3290L deionized water, the flowing of material and water is reverse continuous dynamic flow, obtains 3127kg extracting solution;
(3) centrifugal: by step (2) gained 3127kg extracting solution, 23 DEG C are cooled to rapidly through board frame type heat-exchanger, then first spiral centrifugal is carried out with horizontal spiral centrifuge with centrifugation rate 3000r/min, carry out tubular type with tubular-bowl centrifuge with centrifugation rate 12000r/min more centrifugal, obtain 3122kg centrifugate;
(4) macroporous resin adsorption is separated: by step (3) gained 3122kg centrifugate sodium carbonate adjust ph to 10.63, then the chromatography column (blade diameter length ratio 1:5) crossing filling DM-130 macroporous adsorbent resin carries out upper prop absorption, the flow velocity of upper prop effluent liquid is 0.75BV/h, 2.5h is left standstill after absorption, then wash with deionized water, the flow velocity of deionized water is 2.5BV/h, being washed to effluent liquid is micro-yellow, and to measure pH value be till 7.07, wash-out is carried out again with the ethanolic soln that volume fraction is 70%, the elution flow rate of ethanolic soln is 1.0BV/h, the elution volume of ethanolic soln is 3BV, collecting 1.25 ~ 3.0BV section is target elutriant,
(5) ultrafiltration: the target elutriant molecular weight cut-off that step (4) is collected be 4000 rolling ultrafiltration membrane carry out ultrafiltration, obtain ultrafiltrated;
(6) concentrated: by step (5) gained ultrafiltrated at 76 DEG C, vacuum tightness is under-0.06 ~-0.04MPa, and the sharp degree of vacuum concentration to hundred is 26, obtains concentrated solution;
(7) crystallization and recrystallization: adding methyl alcohol to the volume fraction of methyl alcohol in step (6) gained concentrated solution is 85%, then at temperature 1 DEG C, crystallization, repeat crystallization again 2 times, each crystallization time is 11h, and by crystal at 55 DEG C, vacuum tightness is under-0.09 ~-0.06MPa, carry out vacuum-drying 13h, obtain Rubusoside product 27.05kg.
Detect through HPLC, the product purity of Rubusoside is 99.23%, and yield is 5.41%.
embodiment 4
(1) pre-treatment: by sweet for the 500kg of drying tea raw material (Rubusoside content is 6.44%) removal of impurities, pulverizes, and crosses 40 mesh sieves, obtains sweet tea raw material powder;
(2) microwave counter current extracts: by sweet for step (1) gained 500kg tea raw material powder at 78 DEG C, microwave power is 850w, and frequency is under 5000MHz, carries out microwave counter current extract 57min with 3300L deionized water, the flowing of material and water is reverse continuous dynamic flow, obtains 3131kg extracting solution;
(3) centrifugal: by step (2) gained 3131kg extracting solution, 21 DEG C are cooled to rapidly through board frame type heat-exchanger, then first spiral centrifugal is carried out with horizontal spiral centrifuge with centrifugation rate 4000r/min, carry out tubular type with tubular-bowl centrifuge with centrifugation rate 13000r/min more centrifugal, obtain 3125kg centrifugate;
(4) macroporous resin adsorption is separated: by step (3) gained 3125kg centrifugate sodium hydroxide adjust ph to 10.87, then the chromatography column (blade diameter length ratio 1:4) crossing filling AB-8 macroporous adsorbent resin carries out upper prop absorption, the flow velocity of upper prop effluent liquid is 0.95BV/h, 3h is left standstill after absorption, then wash with deionized water, the flow velocity of deionized water is 2.3BV/h, being washed to effluent liquid is micro-yellow, and to measure pH value be till 6.93, wash-out is carried out again with the ethanolic soln that volume fraction is 75%, the elution flow rate of ethanolic soln is 1.05BV/h, the elution volume of ethanolic soln is 3BV, collecting 1.25 ~ 3.0BV section is target elutriant,
(5) ultrafiltration: the target elutriant molecular weight cut-off that step (4) is collected be 3500 rolling ultrafiltration membrane carry out ultrafiltration, obtain ultrafiltrated;
(6) concentrated: by step (5) gained ultrafiltrated at 78 DEG C, vacuum tightness is under-0.06 ~-0.04MPa, and the sharp degree of vacuum concentration to hundred is 27, obtains concentrated solution;
(7) crystallization and recrystallization: adding methyl alcohol to the volume fraction of methyl alcohol in step (6) gained concentrated solution is 88%, then at temperature-1 DEG C, crystallization, repeat crystallization again 2 times, each crystallization time is 10.5h, and by crystal at 54 DEG C, vacuum tightness is under-0.09 ~-0.06MPa, carry out vacuum-drying 13.5h, obtain Rubusoside product 26.95kg.
Detect through HPLC, the product purity of Rubusoside is 99.28%, and yield is 5.39%.
Claims (10)
1. an extracting method for high purity Rubusoside, is characterized in that: comprise the following steps:
(1) pre-treatment: by the sweet tea impurity removing of drying, pulverizes, sieves, obtain sweet tea raw material powder;
(2) microwave counter current extracts: sweet for step (1) gained tea raw material powder is carried out microwave counter current extraction, obtains extracting solution;
(3) centrifugal: step (2) gained extracting solution to be carried out centrifugal, obtains centrifugate;
(4) macroporous resin adsorption is separated: by step (3) gained centrifugate adjust ph to 10.0 ~ 11.0, then crosses macroporous resin and carries out upper prop absorption, leave standstill after washing, then carry out wash-out with hydrophilic solvent, collect target elutriant;
(5) ultrafiltration: the target elutriant that step (4) is collected is carried out ultrafiltration, obtains ultrafiltrated;
(6) concentrated: it is 25 ~ 28 that step (5) gained ultrafiltrated is concentrated into hundred sharp degree, obtains concentrated solution;
(7) crystallization and recrystallization: adding organic solvent to the volume fraction of organic solvent in step (6) gained concentrated solution is 80 ~ 90%, then carries out crystallization and recrystallization, dry, obtain Rubusoside product.
2. the extracting method of high purity Rubusoside according to claim 1, is characterized in that: in step (2), and the temperature that described microwave counter current extracts is 70 ~ 90 DEG C, and the time is 40 ~ 60min, and the power of microwave is 700 ~ 900w, and frequency is 5000 ~ 7000MHz; Extraction solvent is deionized water, and consumption is 6 ~ 7 times of sweet tea raw materials quality.
3. the extracting method of high purity Rubusoside according to claim 1 or 2, is characterized in that: in step (3), carry out centrifugal before, extracting solution, first through board frame type heat-exchanger, is cooled to 20 ~ 25 DEG C.
4. according to the extracting method of the described high purity Rubusoside of one of claims 1 to 3, it is characterized in that: in step (3), described centrifugal elder generation carries out spiral centrifugal with centrifugation rate 3000 ~ 5000r/min, then it is centrifugal to carry out tubular type with centrifugation rate 12000 ~ 14000r/min.
5. according to the extracting method of the described high purity Rubusoside of one of Claims 1 to 4, it is characterized in that: in step (4), by sodium hydroxide or sodium carbonate adjust ph; Described macroporous resin is D101, AB-8 or DM-130, and the blade diameter length ratio of resin column is 1:4 ~ 6; The flow velocity of described upper prop effluent liquid is 0.5 ~ 1.0BV/h.
6. according to the extracting method of the described high purity Rubusoside of one of Claims 1 to 5, it is characterized in that: in step (4), the described standing time is 2 ~ 3h; During described washing, the flow velocity of water is 2 ~ 3BV/h, be washed to effluent liquid be micro-yellow and pH value is 6.80 ~ 7.20 time till.
7. according to the extracting method of the described high purity Rubusoside of one of claim 1 ~ 6, it is characterized in that: in step (4), described hydrophilic solvent is the ethanolic soln of volume fraction 60 ~ 80%, the elution flow rate of hydrophilic solvent is 0.75 ~ 1.25BV/h, the elution volume of hydrophilic solvent is 3BV, and collection section is 1.25 ~ 3.0BV.
8. according to the extracting method of the described high purity Rubusoside of one of claim 1 ~ 7, it is characterized in that: in step (5), described ultrafiltration adopts rolling ultrafiltration membrane, and the molecular weight cut-off of ultra-filtration membrane is 3000 ~ 5000.
9. according to the extracting method of the described high purity Rubusoside of one of claim 1 ~ 8, it is characterized in that: in step (6), described simmer down to vacuum concentration, temperature is 70 ~ 80 DEG C, and vacuum tightness is-0.06 ~-0.04MPa.
10. according to the extracting method of the described high purity Rubusoside of one of claim 1 ~ 9, it is characterized in that: in step (7), described organic solvent is methyl alcohol or ethanol; The temperature of described crystallization and recrystallization is-2 ~ 3 DEG C, and every subcrystalline time is 10 ~ 12h; Described drying is vacuum-drying, and temperature is 50 ~ 60 DEG C, and vacuum tightness is-0.09 ~-0.06MPa, and the time is 12 ~ 16h.
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| CN106632540A (en) * | 2016-10-27 | 2017-05-10 | 广西金秀香料香精有限责任公司 | Extraction method of rubusoside |
| CN107556350A (en) * | 2017-10-12 | 2018-01-09 | 江南大学 | Rubusoside crystal, its preparation method, food compositions and application with crystal formation A forms |
| CN108276462A (en) * | 2017-06-19 | 2018-07-13 | 桂林莱茵生物科技股份有限公司 | A kind of Rubusoside preparation method |
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| CN113603704A (en) * | 2021-08-30 | 2021-11-05 | 湖南华诚生物资源股份有限公司 | Enzymatic preparation method for separating ellagic acid from byproducts of rubusoside production |
| CN113637038A (en) * | 2021-08-24 | 2021-11-12 | 湖南华诚生物资源股份有限公司 | Method for extracting sweet tea glycoside and sweet tea polyphenol without bitter taste from sweet tea leaves |
| CN113831374A (en) * | 2021-11-08 | 2021-12-24 | 湖南华诚生物资源股份有限公司 | Method for crystallizing rubusoside |
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| CN109717445B (en) * | 2019-01-30 | 2022-10-18 | 湖南绿蔓生物科技股份有限公司 | Sweet taste composition and preparation method and application thereof |
| CN110078775A (en) * | 2019-05-08 | 2019-08-02 | 湖南华诚生物资源股份有限公司 | The environment-protection production method of high-content Rubusoside, sweet tea tannins |
| CN110229201A (en) * | 2019-06-25 | 2019-09-13 | 浙江天草生物科技股份有限公司 | A kind of process preparing high-purity steviosides RM |
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| CN113637038B (en) * | 2021-08-24 | 2022-06-21 | 湖南华诚生物资源股份有限公司 | Method for extracting sweet tea glycoside and sweet tea polyphenol without bitter taste from sweet tea leaves |
| CN113603704A (en) * | 2021-08-30 | 2021-11-05 | 湖南华诚生物资源股份有限公司 | Enzymatic preparation method for separating ellagic acid from byproducts of rubusoside production |
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